Coloration of textile materials



Patented Nov. 7, 1939 UNITED STATES PATENT OFFICE- Spondon, near Derby,England, assignors to Celanese Corporation of America, a corporation ofDelaware No Drawing. Application October 20, 1937, Se-

rial No. 170,053. In Great Britain November 9,

7 Claims.

This invention relates to improvements in the coloration of textilematerials and particularly to improvements in the coloration of mixedtextile materials containing filaments or fibres of organic derivativesof cellulose and other filaments or fibres, for example cotton fibres.

According to the present invention mixed textile materials containingfilaments, yarns or the like of organic derivatives of cellulose andother 10 filamentary constitutents are solid or cross-dyed byimpregnating the materials with diazotisable bases, includingdiazotisable dyestuffs, which, when diazotised and coupled, formdyestufls both for the organic derivative of cellulose constituents andfor the other constituents, and then effecting diazotisation andcoupling of the diazotised bases. Preferably the coupling components forthe organic derivative of. cellulose constituents are incorporated inthe materials before diazotisation.

With suitable components, coupling to form the dyestuff for the organicderivative of cellulose materials may take place in the cold, e. g.simultaneously with diazotisation. In other cases it may be desirable totreat the materials at an increased temperature, e. g. 60 to 80 C., inthe presence of the coupling component after formation of the dyestufffor the cotton or other constituent has been effected at a lowertemperature, e. g. 10 to 20 C.

- While it is preferable to incorporate the coupling component for theorganic derivative of cellulose constituent in the materials beforediazotisation this is not essential and if desired I the whole of thecoupling component or components may be introduced into thefabric orother material after diazotisation. In ithls case 'boric acid or othersihtable buffering agent may be introduced into the medium containingthe coupling component, after cold coupling of the it! diazo compound onthe cotton fibre has been effected, in order to assist the coupling ofthe diazo compound on the cellulose acetate or other organic derivativeof cellulose filaments during a treatment at raised temperature.

The following are examples of the dyeing of mixed fabrics according tothe process of the present invention:--

Example 1 60 A cellulose acetate-cotton woven fabric is introduced intoa dyebath containing about 3% of a 10% paste containing1-amino-3-methoxy benzene-4azo-dimethylaniline, 0.4% of a 10% pastecontaining 4-nitro 2-methoxy amino benzene, about 10% of Chlorazol BlackB. H. (Color Index No. 401), about 1% of naphthol A. s., 0.3% of causticsoda and 1% of boric acid. The dyebath ratio is about :1. and theinitial temperature is C., the temperature being raised during an hourto about 80 C. Two additions 5 of of Glaubers salt are made during thetreatment. After this treatment the fabric is washed off and diazotisedat 10-20 C. for 30 minutes in a 30:1 bath containing about 5% of sodiumnitrite and 20% of formic acid. It is then washed off and introducedinto a 30:1 bath containing about 1% of naphthol A. S. and 0.3% causticsoda and is worked first for about 30 minutes at a temperature of 10-15"C. to form the cotton dyestufi and then for a further 30 minutes 15 at atemperature of 75 C. to form the cellulose acetate dyestuif. The fabricis then introduced into a cold soap bath having a soap concentration ofabout 0.25% and containing about 3% of soda ash, the temperature beingraised to 75 C. during about half an hour. The fabric is then washed offand dried.

The proportions of reagents given above are all based on the weight ofthe fabric except where otherwise stated.

Example 2 A mixed cellulose acetate viscose fabric is dyed in a bathcontaining 10% of ortho-methoxy benzene azoa-naphthylamine and 4% ofdiazo fast yellow 3GL, exhaustion being assisted, if necessary, by theaddition of salt. The material is then diazotised in the cold, rinsedand treated in a bath containing 2% of p-naphthol at room temperature,the temperature being gradually raised to about C.

In this manner a dyed mixed fabric is obtained in which the celluloseacetate yarn is dyed a deep purple and the viscose yarn a reddishorange.

Example 3 A mixed cellulose acetate viscose fabric is dyed in a bathcontaining the following constituents:

Per cent Fast red RL base 1 Naphthol ASLT 2 Sodium hydroxide 0.5Chlorazol Black BH. (Color Index No. 401)- 10 The alkali is bufferedwith boric acid or glucose and the material is treated for about an hourat to C. with the addition of 50% of. Glaubers salt to increase theexhaustion of the cotton color. After rinsing the material is introducedinto a 15:1 bath containing 5% of sodium nitrite and 20% of formic acidand worked cold for 30 minutes. Diazotisation of the bases and couplingon the cellulose acetate take place in this bath, a deep red color beingdeveloped after about 30 minutes. The material is then rinsed andintroduced into a fresh bath, containing one gran; per litre of soda ashand 1% of naphthol ASLT dissolved in 0.25% of caustic soda, to completecoupling on the viscose.

In this manner a dyed mixed fabric is obtained in which the celluloseacetate constituents are colored a deep red and the viscose constituentsa navy blue, coupling on both the constituents being completed at atemperature of about 30 C.

Example 4 A cellulose acetateviscose fabric is dyed in a similar mannerto that described in Example 3 using a bath containing the followingconstituents:

Per cent Fast red RL base 1 Naphthol ASLT 2 Caustic soda 0.5 Diazo fastgreen GFL 3 After treatment with the above liquor the fabric isintroduced into a diazotising bath for about 30 minutes in whichdiazotisation is effected and coupling on the cellulose acetateconstituents takes place. The fabric is then rinsed and introduced intoa bath containing 1% of phenylmethyl-pyrozolone in which coupling on theviscose' takes place.

In this manner a dyed mixed fabric is obtained in which the celluloseacetate constituents are colored a bright red and the viscoseconstituents green.

In each of the above examples the fabric treated contains about 50% ofeach type of yarn. In Examples 2-4 the proportions of dyestuffs arecalculated on the weights of the respective yarns and the other reagentson the weights of the fabrics, except where otherwise stated.

The process of the present invention is applicable to the coloring ofmixed yarns, fabrics and other textile materials containing constituentsmade of cellulose acetate or other organic derivative of cellulosetogether with other constituents, for example cotton or regeneratedcellulose fibres. The organic derivative of cellulose constituents mayfor example be continuous filaments, obtained for example by theextrusion of a solution of cellulose acetate, spun yarns, made fromstaple fibres obtained for example from such continuous filaments or bythe acetylation of cotton or other cellulosig fibres without destroyingtheir structure, or filamentary materials of relatively high denier suchas straw or slit foil. The process is applicable to the production ofany suitable azo dyestuffs on the mixed mate rials. As examples ofsuitable bases which may be employed may be mentioned o-chloraniline,para-nitraniline, para-nitrobenzene azo-paraxylidine,m-nitro-p-toluidine, o-anisidine, dianisidine, a-naphthylamine,benzidine, and mono aceto-acetyl 4.4 diamino azobenzene, while asexamples of suitable coupling components may be mentioned resorcin,fi-naphthol, anaphthol, amino-phenols and amino-naphthols, oxy-naphthoicacids, ,B-naphthylamine, p.amino diphcnylamine, and fi-keto-acidylarylides, e. g. diaceto acetyl-o-tolidide.

Having described our invention, what we desire to secure by LettersPatent is:

1. Process for the coloration with azo dyestuffs of mixed textilematerials containing filaments, yarns or the like of organic derivativesof cellulose and cellulosic filaments, yarns or the like, whichcomprises impregnating the materials with the diazotizable basecomponent and the couof mixed textile materials containing filaments,

yarns or the like of cellulose acetate and cellulosic filaments, yarnsor the like, which comprises impregnating the materials with thediazotizable base component andthe coupling component of the dyestufffor the cellulose acetate constituent of the materials and with thediazotizable base component of the dyestuff for the cellulosicconstituent of the materials, and then effecting diazotization of thediazotized bases and the coupling of the coupling component for thecellulose derivative dyestufi, and then coupling with a couplingcomponent of the dyestuff for the cellulosic constituents.

3. Process for the coloration with azo dyestuffs of mixed textilematerials containing filaments, yarns or the like of organic derivativesof cellulose and cellulosic filaments, yarns or the like, whichcomprises impregnating the materials with the diazotizablc basecomponent and the coupling component of the dyestuff for the organicderivative of cellulose constituent of the materials and with thediazotizable base component of the dyestuff for thecellulosic-constituents of the materials, then diazotizing the basecomponents, applying a coupling component for the dyestufi" of thecellulosic constituents and coupling the same at about room temperature,and subsequently effecting coupling of the components of the dyestufffor the organic derivative of cellulose constituent at a materiallyhigher tempera ture.

4. Process for the coloration with azo dyestuffs of mixed textileaterials containing filaments, yarns or the like of cellulose acetateand cellulosic filaments, yarns or the like, which comprisesimpregnating the materials with the diazotizable base component and thecoupling componentof the dyestuil for the cellulose acetate constituentof the materials and With the diazotizable base component of thedyestuff for the cellulosic constituent of the materials, thendiazotizing the base components, applying a coupling component for thedyestuff of the cellulosic constituents and coupling the same at aboutroom temperature, and subsequently effecting coupling of the componentsof the dyestuff for the cellulose acetate constituent at a materiallyhigher temperature.

5. Process for the coloration with azo dyestuffs of mixed textilematerials containing filaments, yarns or the like of cellulose acetateand cellulosic filaments, yarns or the like, which comprisesimpregnating the materials with the diazotizable base component and thecoupling component of the dyestuff for the cellulose acetate constituentof the materials and with the diazotizable base component of thedyestuff for the cellulosio constituent of the materials, thendiazotizing the base components, applying a couthe said couplingcomponent being an arylide of 2:3 hydroxynaphthoic acid, and with'thediazotizable base component of the dyestufi for the cellulosicconstituent of the materials, and then efiecting diazotization of thediazotized bases and the coupling of the coupling component for thecellulose derivative dyestuff, and then coupling with a couplingcomponent of the dyestufi forthe cellulosic constituents.

organic derivatives of cellu- 5 '7. Process for the coloration with aZodyestuffs of mixed textile materials containing filaments,

yarns or the like of cellulose acetate and cellulosic filaments, yarnsor the like, which comprises impregnatingthe materials with thediazotizable base component and the coupling component of the dyestufifor the cellulose acetate constituent of the materials, the saidcoupling component beingan'arylide of 2:3 hydroxynaphthoic acid, and

with the diazotizable base component of the dyestufi'ifor the cellulosicconstituent of the matethe dyestufi of at about frooni temperature, andsubsequently efiecting" coupling of the components of theclyestufi'forthe cellulose acetate constituent at a materiallyfhighertemperature. r

GEORGE HOLLAND ELLIS.

CHARLES FINLEY TOPHAM.

rials',-then,diazotizing the base components, applying a cou-plingcomponent for the cellulosicconstituents and coupling the same

